CN115667415B - 激光熔敷用透光性树脂组合物、组合物组合、成型品、以及成型品的制造方法 - Google Patents
激光熔敷用透光性树脂组合物、组合物组合、成型品、以及成型品的制造方法 Download PDFInfo
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- CN115667415B CN115667415B CN202180037763.1A CN202180037763A CN115667415B CN 115667415 B CN115667415 B CN 115667415B CN 202180037763 A CN202180037763 A CN 202180037763A CN 115667415 B CN115667415 B CN 115667415B
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Abstract
本发明提供抑制了着色剂向其它构件的颜色迁移的激光熔敷用透光性树脂组合物、组合物组合、成型品及成型品的制造方法。一种激光熔敷用透光性树脂组合物,其相对于结晶性热塑性树脂100质量份包含增强填料10~120质量份、具有苝骨架的透光性色素0.01~1.0质量份、以及铜化合物、卤化碱金属及氧化铈中的至少一种。
Description
技术领域
本发明涉及激光熔敷用透光性树脂组合物、组合物组合、成型品、以及成型品的制造方法。
背景技术
热塑性树脂容易加工,利用其优异的特性,广泛用于车辆部件、电气/电子设备部件、其它精密仪器部件等。最近,形状复杂的部件也可以用热塑性树脂、特别是结晶性热塑性树脂来制造,在进气歧管这样的具有中空部的部件等的粘接中,具体而言,可以使用粘接剂熔敷、振动熔敷、超声波熔敷、热板熔敷、注射熔敷、激光熔敷技术等各种熔敷技术。
然而,通过粘接剂进行的熔敷除了损失至固化为止的时间以外,还存在周围污染等环境负担的问题。已指出超声波熔敷、热板熔敷等由于振动、热而导致产品发生损伤、磨损粉末、毛边,从而需要进行后处理等的问题。另外,注射熔敷大多数情况下需要特殊的模具、成型机,而且存在材料的流动性差时无法使用等的问题。
另一方面,激光熔敷是将对激光具有透射性(也称为非吸收性、弱吸收性)的树脂构件(以下,有时称为“透射树脂构件”)与对激光具有吸收性的树脂构件(以下,有时称为“吸收树脂构件”)接触、熔敷而使两个树脂构件接合的方法。具体而言,是从透射树脂构件侧对接合面照射激光,利用激光的能量使形成接合面的吸收树脂构件熔融而进行接合的方法。激光熔敷不产生磨损粉末、毛边,对产品的损伤也小,另外,聚酰胺树脂本身是激光透射率较高的材料,因此,聚酰胺树脂产品的基于激光熔敷技术的加工最近受到关注。
上述透射树脂构件通常可以将透光性树脂组合物成型而得到。作为这样的透光性树脂组合物,在专利文献1中公开了一种激光熔敷用树脂组合物,其是相对于(A)聚酰胺树脂100质量份配合(B)23℃的折射率为1.560~1.600的增强填充材料1~150质量份而成的树脂组合物,其中,构成上述(A)聚酰胺树脂中的至少一种的至少一种单体含有芳香环。在专利文献1的实施例中公开了在聚酰胺MXD6与聚酰胺66的混合物、或聚酰胺6I/6T与聚酰胺6的混合物中配合有玻璃纤维和着色剂的树脂组合物。
现有技术文献
专利文献
专利文献1:日本特开2008-308526号公报
发明内容
发明所要解决的问题
这里,随着激光熔敷技术进步,进一步要求新型材料。特别是要求能够在激光熔敷后抑制透射树脂构件中的透光性色素向其它构件(周边构件)发生颜色迁移的材料。
本发明的目的在于解决上述课题,提供抑制了着色剂向其它构件的颜色迁移的激光熔敷用透光性树脂组合物、以及组合物组合、成型品及成型品的制造方法。
解决问题的方法
基于上述课题,本发明人进行了研究,结果发现,通过使用具有苝骨架的透光性色素作为透光性色素,从而解决了上述课题。
具体而言,通过下述方法解决了上述课题。
<1>一种激光熔敷用透光性树脂组合物,其相对于结晶性热塑性树脂100质量份包含增强填料10~120质量份、具有苝骨架的透光性色素0.01~1.0质量份、以及铜化合物、卤化碱金属及氧化铈中的至少一种。
<2>根据<1>所述的树脂组合物,其中,
上述树脂组合物中的镧的含量超过0质量ppm且为40质量ppm以下。
<3>根据<1>或<2>所述的树脂组合物,其包含通过ICP发光分析法测得的镧的含量超过0质量%且为1质量%以下的氧化铈。
<4>根据<1>~<3>中任一项所述的树脂组合物,其中,
树脂组合物中上述氧化铈的含量为0.01~5质量%。
<5>根据<1>~<4>中任一项所述的树脂组合物,其中,
上述结晶性热塑性树脂包含聚酰胺树脂。
<6>根据<5>所述的树脂组合物,其中,
上述聚酰胺树脂包含来自二胺的结构单元和来自二羧酸的结构单元,来自二胺的结构单元的70摩尔%以上来自于苯二甲基二胺,来自二羧酸的结构单元的70摩尔%以上来自于碳原子数4~20的α,ω-直链脂肪族二羧酸。
<7>根据<1>~<6>中任一项所述的树脂组合物,其中,
上述具有苝骨架的透光性色素为颜料。
<8>一种组合物组合,其具有:
<1>~<7>中任一项所述的树脂组合物、和
包含热塑性树脂和光吸收性色素的光吸收性树脂组合物。
<9>一种成型品,其由<1>~<7>中任一项所述的树脂组合物或<8>所述的组合物组合形成。
<10>根据<9>所述的成型品,其为车载相机部件。
<11>一种车载相机,其包含<10>所述的成型品。
<12>一种成型品的制造方法,该方法包括:
对由<1>~<7>中任一项所述的树脂组合物形成的成型品、以及由包含热塑性树脂和光吸收性色素的光吸收性树脂组合物形成的成型品进行激光熔敷。
发明的效果
通过本发明,能够提供抑制了着色剂向其它构件的颜色迁移的激光熔敷用透光性树脂组合物、以及组合物组合、成型品及成型品的制造方法。
具体实施方式
以下,对用于实施本发明的方式(以下,简称为“本实施方式”)详细地进行说明。需要说明的是,以下的本实施方式是用于对本发明进行说明的示例,本发明并不仅限定于本实施方式。
需要说明的是,在本说明书中,“~”以包含记载于其前后的数值作为下限值及上限值的含义而使用。
在本说明书中,只要没有特别说明,则各种物性值及特性值是在23℃下的值。
在本说明书中,ppm是指质量ppm。
本实施方式的激光熔敷用透光性树脂组合物(以下有时简称为“树脂组合物”)包含:结晶性热塑性树脂、增强填料、具有苝骨架的透光性色素、以及铜化合物、卤化碱金属及氧化铈中的至少一种,其中,相对于结晶性热塑性树脂100质量份,包含增强填料10~120质量份,包含具有苝骨架的透光性色素0.01~1.0质量份。通过设为这样的构成,能够有效地抑制透光性色素向其它构件的颜色迁移。
在铜化合物、卤化碱金属及氧化铈中,本实施方式的树脂组合物优选至少包含氧化铈。
<结晶性热塑性树脂>
本实施方式的树脂组合物包含结晶性热塑性树脂。通过使用结晶性热塑性树脂,可得到具备结晶性热塑性树脂原本具有的激光熔敷所要求的性能的树脂组合物。具体而言,可示例出结晶性热塑性树脂所具有的低吸水率、不易因模具温度等而产生热收缩率偏差、高机械强度等。
作为结晶性热塑性树脂,可示例出聚酰胺树脂、结晶性聚酯树脂等,优选为聚酰胺树脂。
作为聚酰胺树脂,是以通过内酰胺的开环聚合、氨基羧酸的缩聚、二胺与二元酸的缩聚而得到的酰胺作为重复单元的高分子,具体可举出:聚酰胺6、聚酰胺11、聚酰胺12、聚酰胺46、聚酰胺66、聚酰胺610、聚酰胺612、聚酰胺1010、聚酰胺1012、聚酰胺6I、聚酰胺6/66、聚酰胺6T/6I、聚酰胺6/6T、聚酰胺66/6T、聚酰胺66/6T/6I、聚三甲基六亚甲基对苯二甲酰胺、聚双(4-氨基环己基)甲烷月桂酰胺、聚双(3-甲基-4-氨基环己基)甲烷月桂酰胺、聚十一亚甲基六氢对苯二甲酰胺、后述的苯二甲基二胺类聚酰胺树脂等。需要说明的是,上述“I”表示间苯二甲酸成分,“T”表示对苯二甲酸成分。
作为本实施方式中使用的聚酰胺树脂,可以考虑这些聚酰胺树脂所具有的各种特性和作为目标的成型品的用途等而选择适当的聚酰胺树脂。
在上述的聚酰胺树脂中,优选为包含来自二胺的结构单元和来自二羧酸的结构单元的聚酰胺树脂(苯二甲基二胺类聚酰胺树脂),其中,来自二胺的结构单元的70摩尔%以上来自于苯二甲基二胺,来自二羧酸的结构单元的70摩尔%以上来自于碳原子数4~20的α,ω-直链脂肪族二羧酸。
本实施方式中使用的苯二甲基二胺类聚酰胺树脂中,优选来自二胺的结构单元的80摩尔%以上、更优选为90摩尔%以上、进一步优选为95摩尔%以上、更进一步优选为99摩尔%以上来自于苯二甲基二胺。
来自苯二甲基二胺的结构单元优选为来自间苯二甲基二胺的结构单元和/或来自对苯二甲基二胺的结构单元,更优选包含50~90摩尔%的间苯二甲基二胺和10~50摩尔%的对苯二甲基二胺(但是,总计不超过100摩尔%),进一步优选包含60~80摩尔%的间苯二甲基二胺和20~40摩尔%的对苯二甲基二胺。在本实施方式所使用的苯二甲基二胺类聚酰胺树脂中,优选来自苯二甲基二胺的结构单元的95摩尔%以上(优选为99摩尔%以上)为来自间苯二甲基二胺的结构单元和/或来自对苯二甲基二胺的结构单元。
作为可以用作苯二甲基二胺类聚酰胺树脂的原料二胺成分的除苯二甲基二胺以外的二胺,可以示例出:四亚甲基二胺、五亚甲基二胺、2-甲基戊二胺、六亚甲基二胺、七亚甲基二胺、八亚甲基二胺、九亚甲基二胺、十亚甲基二胺、十二亚甲基二胺、2,2,4-三甲基六亚甲基二胺、2,4,4-三甲基六亚甲基二胺等脂肪族二胺;1,3-双(氨基甲基)环己烷、1,4-双(氨基甲基)环己烷、1,3-二氨基环己烷、1,4-二氨基环己烷、双(4-氨基环己基)甲烷、2,2-双(4-氨基环己基)丙烷、双(氨基甲基)萘烷、双(氨基甲基)三环癸烷等脂环式二胺;双(4-氨基苯基)醚、对苯二胺、双(氨基甲基)萘等具有芳香环的二胺等,可以使用一种或混合两种以上使用。
本实施方式中使用的苯二甲基二胺类聚酰胺树脂中,来自二羧酸的结构单元的70摩尔%以上、优选为75摩尔%以上、更优选为85摩尔%以上、进一步优选为95摩尔%以上、更进一步优选为99摩尔%以上来自于碳原子数4~20的α,ω-直链脂肪族二羧酸。
作为碳原子数为4~20的α,ω-直链脂肪族二羧酸,可示例出丁二酸、戊二酸、己二酸、癸二酸、十一烷二酸、十二烷二酸等,优选为己二酸和/或癸二酸。碳原子数为4~20的α,ω-直链脂肪族二羧酸可以使用一种或混合两种以上使用。
作为上述碳原子数4~20的α,ω-直链脂肪族二羧酸以外的二羧酸成分,可示例出间苯二甲酸、对苯二甲酸、邻苯二甲酸等苯二甲酸化合物、1,2-萘二甲酸、1,3-萘二甲酸、1,4-萘二甲酸、1,5-萘二甲酸、1,6-萘二甲酸、1,7-萘二甲酸、1,8-萘二甲酸、2,3-萘二甲酸、2,6-萘二甲酸、2,7-萘二甲酸这样的萘二甲酸的异构体等,可以使用一种或混合两种以上使用。
作为苯二甲基二胺类聚酰胺树脂的一个实施方式,优选作为原料的苯二甲基二胺包含50~90摩尔%的间苯二甲基二胺和10~50摩尔%的对苯二甲基二胺,且碳原子数4~20的α,ω-直链脂肪族二羧酸包含己二酸和/或癸二酸。进一步优选原料二胺的90摩尔%以上为苯二甲基二胺,上述苯二甲基二胺以总计99摩尔%以上包含60~80摩尔%的间苯二甲基二胺和40~20摩尔%的对苯二甲基二胺,且α,ω-直链脂肪族二羧酸的90摩尔%以上为己二酸和/或癸二酸。
需要说明的是,本实施方式中使用的苯二甲基二胺类聚酰胺树脂以来自二胺的结构单元和来自二羧酸的结构单元作为主成分而构成,但并不完全排除除此以外的结构单元,当然也可以包含来自于ε-己内酰胺、月桂内酰胺等内酰胺类、氨基己酸、氨基十一烷酸等脂肪族氨基羧酸类的结构单元。这里,主成分是指,构成苯二甲基二胺类聚酰胺树脂的结构单元中,来自二胺的结构单元和来自二羧酸的结构单元的总计数量在全部结构单元中最多。在本实施方式中,优选苯二甲基二胺类聚酰胺树脂中的来自二胺的结构单元和来自二羧酸的结构单元的总计占据全部结构单元的90%以上、更优选占据95%以上。
本实施方式的树脂组合物优选以树脂组合物的30质量%以上的比例包含结晶性热塑性树脂(优选为聚酰胺树脂、更优选为苯二甲基二胺类聚酰胺树脂),更优选以35质量%以上的比例包含,进一步优选以40质量%以上的比例包含,更进一步优选以45质量%以上的比例包含。另外,作为上述结晶性热塑性树脂的含量的上限值,优选为80质量%以下,更优选为75质量%以下。
本实施方式的树脂组合物可以仅包含一种结晶性热塑性树脂,也可以包含两种以上。在包含两种以上的情况下,优选总计量为上述范围。
<增强填料>
相对于结晶性热塑性树脂100质量份,本实施方式的树脂组合物以10~120质量份的比例包含增强填料。通过以上述比例包含增强填料,可以实现高机械强度。需要说明的是,本实施方式中的增强填料不包含相当于后面说明的氧化铈、成核剂的成分。
作为本实施方式中的增强填料,具有使配合于树脂中而得到的树脂组合物的机械性质提高的效果,可以使用常用的塑料用增强材料。增强填料可以是有机物,也可以是无机物,优选为无机物。增强填料可以优选使用玻璃纤维、碳纤维、玄武岩纤维、硅灰石、钛酸钾纤维等纤维状的增强填料。另外,也可以使用碳酸钙、氧化钛、长石类矿物、粘土、有机化粘土、玻璃珠等粒状或无定形的填充剂等填充剂;玻璃片、云母、石墨等鳞片状的增强材料。其中,从机械强度、刚性及耐热性的方面出发,优选使用纤维状的填充剂、特别是玻璃纤维。作为玻璃纤维,可以使用圆形截面形状的玻璃纤维或异形截面形状的玻璃纤维中的任意玻璃纤维。
增强填料更优选使用通过偶联剂等表面处理剂进行了表面处理后的增强填料。附着有表面处理剂的玻璃纤维的耐久性、耐湿热性、耐水解性、耐热冲击性优异,因此优选。
玻璃纤维包含A玻璃、C玻璃、E玻璃、S玻璃、R玻璃、M玻璃、D玻璃等玻璃组成,特别优选为E玻璃(无碱玻璃)。
玻璃纤维是指,在长度方向上切断成直角的截面形状为正圆状、多边形状且呈现纤维状外观的玻璃纤维。
本实施方式的树脂组合物中使用的玻璃纤维可以是单纤维、或者将多根单纤维捻合而成的纤维。
玻璃纤维的形态可以是将单纤维或多根单纤维捻合成的纤维连续卷取而成的“玻璃粗纱”、整齐切成长度1~10mm的“短切原丝”、粉碎成长度10~500μm的“碾磨纤维”等中的任意纤维。作为上述玻璃纤维,由Asahi Fiber Glass公司以“Glassron Chopped Strand”、“Glassron Milled Fiber”的商品名销售,可以容易地获得。玻璃纤维还可以组合使用形态不同的纤维。
另外,本实施方式中使用的玻璃纤维的截面可以为圆形,也可以非圆形。通过使用截面为非圆形的玻璃纤维,可以更有效地抑制得到的成型品的翘曲。另外,在本实施方式中,即使使用截面为圆形的玻璃纤维,也可以有效地抑制翘曲。
相对于结晶性热塑性树脂100质量份,本实施方式的树脂组合物中的增强填料的含量为10质量份以上,优选为20质量份以上,进一步优选为30质量份以上,进一步优选为40质量份以上。关于上限值,相对于结晶性热塑性树脂100质量份,优选为120质量份以下,更优选为110质量份以下。
本实施方式的树脂组合物中的增强填料的含量优选为树脂组合物的20质量%以上,更优选为25质量%以上。关于上限值,优选为70质量%以下,更优选为65质量%以下,进一步优选为60质量%以下,更进一步优选为55质量%以下。
本实施方式的树脂组合物可以仅包含一种增强填料,也可以包含两种以上。在包含两种以上的情况下,总计量为上述范围。需要说明的是,本实施方式中的增强填料的含量中包含集束剂及表面处理剂的量。
<具有苝骨架的透光性色素>
本实施方式的树脂组合物相对于结晶性热塑性树脂100质量份以0.01~1.0质量份的比例包含具有苝骨架的透光性色素。通过配合具有苝骨架的透光性色素,能够有效地抑制向其它构件(特别是吸收树脂构件)的颜色迁移。
本实施方式中使用的透光性色素优选为黑色色素、黑紫色素等以人类视觉可观察为黑色的色素。另外,透光性色素中包含如下色素:以使总计成为100质量%的方式配合结晶性热塑性树脂(优选为聚酰胺树脂、更优选为苯二甲基二胺类聚酰胺树脂)的至少一种、玻璃纤维30质量%、以及色素(被认为透光性色素的色素)0.2质量%,测定波长1070nm下的透光率时透射率成为20%以上的色素。
透光性色素可以是染料,也可以是颜料,优选为颜料。
作为具有苝骨架的色素,可示例出BASF Color&Effect Japan株式会社制、Spectrasence K0087(旧名:Lumogen(注册商标)Black K0087、Lumogen Black FK4280)、Spectrasence K0088(旧名:Lumogen Black K0088、Lumogen Black FK4281)等。
本实施方式的树脂组合物相对于结晶性热塑性树脂100质量份包含具有苝骨架的透光性色素0.01质量份以上,优选为0.05质量份以上,进一步优选为0.08质量份以上,更进一步优选为0.10质量份以上,更进一步优选为0.15质量份以上,更进一步优选为0.18质量份以上,特别优选为0.20质量份以上。另外,本实施方式的树脂组合物相对于结晶性热塑性树脂100质量份包含具有苝骨架的透光性色素1.0质量份以下,优选为0.8质量份以下,进一步优选为0.6质量份以下,更进一步优选为0.5质量份以下,更进一步优选为0.45质量份以下。
本实施方式的树脂组合物可以仅包含一种具有苝骨架的透光性色素,也可以包含两种以上。在包含两种以上的情况下,优选总计量为上述范围。
本实施方式的树脂组合物也可以包含具有苝骨架的透光性色素以外的其它色素,但优选实质上不包含。实质上不包含是指,例如,其它色素的含量小于具有苝骨架的透光性色素的含量的1质量%。
<铜化合物>
本实施方式的树脂组合物可以包含铜化合物。通过使用铜化合物,能够实现显著优异的耐热老化性。
作为本实施方式中使用的铜化合物,可示例出:卤化铜(例如碘化铜、溴化铜、氯化铜)及乙酸铜,优选选自碘化亚铜、碘化铜、溴化亚铜、溴化铜、乙酸亚铜、乙酸铜、氯化亚铜及氯化铜,更优选选自碘化亚铜、乙酸铜及氯化亚铜,进一步优选为碘化亚铜。
另外,铜化合物优选与后述的卤化碱金属组合使用。在将铜化合物与卤化碱金属组合的情况下,优选为铜化合物∶卤化碱金属的1:1~1:15(质量比)的混合物,进一步优选为1:1~1:5的混合物,更进一步优选为1:2~1:4的混合物。
关于将铜化合物与卤化碱金属组合的情况,也可以参照日本特表2013-513681号公报第0046~0048段的记载,将这些内容引入本说明书。
本实施方式的树脂组合物中的铜化合物的比例优选为0.01~1质量%,更优选为0.05质量%以上,而且更优选为0.5质量%以下。
本实施方式的树脂组合物可以仅包含一种铜化合物,也可以包含两种以上。在包含两种以上的情况下,优选总计量为上述范围。
<卤化碱金属>
本实施方式的树脂组合物可以包含卤化碱金属。通过使用卤化碱金属,存在耐热老化性及耐湿热性进一步提高的倾向。
本实施方式中使用的卤化碱金属是指碱金属的卤化物。作为碱金属,优选为钾及钠,更优选为钾。另外,作为卤原子,优选为碘、溴、氯,更优选为碘。作为本实施方式中使用的卤化碱金属的具体例,可示例出碘化钾、溴化钾、氯化钾及氯化钠,优选为碘化钾。
本实施方式的树脂组合物中的卤化碱金属的比例优选为0.01~1质量%,更优选为0.1质量%以上,而且更优选为0.5质量%以下。
本实施方式的树脂组合物可以包含仅一种卤化碱金属,也可以包含两种以上。在包含两种以上的情况下,优选总计量为上述范围。
<氧化铈>
本实施方式的树脂组合物优选包含氧化铈。通过包含氧化铈,即使在高温湿热下放置后,也能够有效地抑制向其它构件(特别是作为激光熔敷的对象的吸收树脂构件)的颜色迁移。此外,氧化铈的莫氏硬度比较低,因此,能够不易对玻璃纤维等增强填料造成损伤。
本实施方式中的氧化铈是指纯度为90质量%以上的氧化铈。即,氧化铈中可以包含杂质。本实施方式中使用的氧化铈优选为通过ICP发光分析法测得的镧的含量超过0质量%且为1质量%以下的氧化铈,更优选为通过ICP发光分析法测得的镧的含量为0.01~0.7质量%的氧化铈,进一步优选为通过ICP发光分析法测得的镧的含量为0.02~0.4质量%的氧化铈,更进一步优选为通过ICP发光分析法测得的镧的含量为0.05~0.2质量%的氧化铈。通过设为这样的范围,能够更有效地抑制向其它构件的颜色迁移。
这样,能够通过使用以微量的比例包含镧的氧化铈而容易地在树脂组合物中配合期望量的镧。
在本实施方式中,氧化铈中的铈的含量优选为73质量%以上,更优选为75质量%以上,进一步优选为77质量%以上。另外,上述氧化铈的含量的上限优选为85质量%以下,更优选为83质量%以下,进一步优选为80质量%以下。
本实施方式中使用的氧化铈的中值粒径(基于激光衍射散射法的粒度)优选为3μm以下。上述中值粒径的下限例如为0.1μm以上。
通过使用具有上述中值粒径的氧化铈,能够有效地抑制对增强填料的损伤,可得到机械强度更优异的树脂组合物。
在树脂组合物中,本实施方式的树脂组合物中的氧化铈的含量优选为0.01质量%以上,更优选为0.05质量%以上。另外,作为树脂组合物中的氧化铈的含量的上限值,优选为5质量%以下,进一步优选为4质量%以下,更进一步优选为3质量%以下,更进一步优选为2质量%以下。
<脱模剂>
本实施方式的树脂组合物可以包含脱模剂。
作为脱模剂,可列举例如:脂肪族羧酸、脂肪族羧酸的盐、脂肪族羧酸与醇形成的酯、数均分子量200~15000的脂肪族烃化合物、聚硅氧烷类硅油、酮蜡、Light Amide等,优选为脂肪族羧酸、脂肪族羧酸的盐、脂肪族羧酸与醇形成的酯,更优选为脂肪族羧酸的盐。
脱模剂的详细内容可以参照日本特开2018-095706号公报的第0055~0061段的记载,将这些内容引入本说明书。
在本实施方式的树脂组合物包含脱模剂的情况下,其含量在树脂组合物中优选为0.05~3质量%,更优选为0.1~0.8质量%,进一步优选为0.2~0.6质量%。
本实施方式的树脂组合物可以仅包含一种脱模剂,也可以包含两种以上脱模剂。在包含两种以上的情况下,优选总计量为上述范围。
<成核剂>
本实施方式的树脂组合物可以包含成核剂。通过配合成核剂,可促进结晶化,变得易于凝固,因此能够改善成型周期。成核剂只要是在熔融加工时未熔融、且在冷却过程中能够形成结晶核的物质即可,没有特别限定,其中,优选为滑石及碳酸钙,更优选为滑石。
成核剂的数均粒径的下限值优选为0.1μm以上,更优选为1μm以上,进一步优选为3μm以上。成核剂的数均粒径的上限值优选为40μm以下,更优选为30μm以下,进一步优选为28μm以下,更进一步优选为15μm以下,进一步更优选为10μm以下。
本实施方式的树脂组合物中的成核剂的比例优选为0.01~1质量%,更优选为0.1质量%以上,而且更优选为0.5质量%以下。
本实施方式的树脂组合物可以仅包含一种成核剂,也可以包含两种以上。在包含两种以上的情况下,优选总计量为上述范围。
<其它成分>
在不脱离本实施方式的主旨的范围内,本实施方式的树脂组合物可以包含其它成分。作为这样的添加剂,可举出光稳定剂、抗氧剂、紫外线吸收剂、荧光增白剂、防滴落剂、抗静电剂、防雾剂、防粘连剂、流动性改良剂、增塑剂、分散剂、抗菌剂、阻燃剂等。这些成分可以仅使用一种,也可以组合使用两种以上。
需要说明的是,对于本实施方式的树脂组合物而言,以各成分的总计成为100质量%的方式调整结晶性热塑性树脂、增强填料、具有苝骨架的透光性色素、以及铜化合物、卤化碱金属及氧化铈中的至少一种、以及其它添加剂的含量等。在本实施方式中,示例出结晶性热塑性树脂、增强填料、具有苝骨架的透光性色素、以及铜化合物、卤化碱金属及氧化铈中的至少一种、成核剂、脱模剂的总计占据树脂组合物的99质量%以上的方式。
<树脂组合物中的镧的含量>
本实施方式的树脂组合物的镧的含量优选超过0质量ppm且为150质量ppm以下。通过这样包含微量的镧,即使在高温高湿下放置后,也能够更有效地抑制颜色迁移。另外,通过设为150质量ppm以下、特别是40质量ppm以下,能够将在高温高湿下放置后的拉伸强度保持为较高水平。
上述树脂组合物中的镧的含量的下限值优选为0.01质量ppm以上,更优选为0.05质量ppm以上,进一步优选为0.1质量ppm以上,更进一步优选为0.5质量ppm以上,更进一步优选为0.8质量ppm以上,更进一步优选为1质量ppm以上,特别优选为2质量ppm以上。
另外,上述树脂组合物中的镧的含量的上限值优选为40质量ppm以下,更优选为30质量ppm以下,进一步优选为25质量ppm以下,更进一步优选为20质量ppm以下,更进一步优选为15质量ppm以下,更进一步优选为12质量ppm以下,特别优选为8质量ppm以下,更特别优选为5质量ppm以下。
在本实施方式的树脂组合物中,通常以氧化铈中包含的镧的形式配合镧。
<树脂组合物的制造方法>
本实施方式的树脂组合物的制造方法没有特别限制,优选为使用具有可以从排气口脱气的设备的单螺杆或双螺杆挤出机作为混炼机的方法。可以将上述结晶性热塑性树脂、增强填料、透光性色素、碘化铜、碘化钾及氧化铈的至少一种、以及根据需要配合的其它添加剂一起供给至混炼机,也可以在供给结晶性热塑性树脂后,依次供给其它配合成分。为了抑制在混炼时破碎,优选从挤出机的中途供给增强填料。另外,也可以将选自各成分中的两种以上成分预先混合、混炼。
在本实施方式中,对于透光性色素而言,可以预先制备用结晶性热塑性树脂等进行了母炼胶化后的材料,然后与其它成分(结晶性热塑性树脂、增强填料、透光性色素、碘化铜、碘化钾及氧化铈中的至少一种等)混炼,从而得到本实施方式的树脂组合物。
使用了本实施方式的树脂组合物的成型品的制造方法没有特别限制,可以应用对于热塑性树脂通常使用的成型方法、即注塑成型、中空成型、挤出成型、加压成型等成型方法。在该情况下,由于流动性良好,特别优选的成型方法是注塑成型。在注塑成型时,优选将料筒温度控制为250~300℃。
<组合物组合>
优选使用本实施方式的树脂组合物、以及包含热塑性树脂和光吸收性色素的光吸收性树脂组合物作为组合物组合、特别是用于利用激光熔敷制造成型品(激光熔敷物)的组合物组合。
即,组合物组合中包含的本实施方式的树脂组合物发挥作为透光性树脂组合物的作用,由上述透光性树脂组合物形成的成型品成为在激光熔敷时对激光的透射树脂构件。另一方面,由光吸收性树脂组合物形成的成型品成为在激光熔敷时对激光的吸收树脂构件。
<<光吸收性树脂组合物>>
本实施方式中使用的光吸收性树脂组合物包含热塑性树脂和光吸收性色素。此外,也可以包含增强填料等其它成分。
热塑性树脂可示例出聚酰胺树脂、烯烃类树脂、乙烯基类树脂、苯乙烯类树脂、丙烯酸类树脂、聚苯醚树脂、聚酯树脂、聚碳酸酯树脂、聚缩醛树脂等,从与透光性树脂组合物(本实施方式的树脂组合物)的相容性良好的方面考虑,特别优选为结晶性热塑性树脂,更优选为聚酰胺树脂、结晶性聚酯树脂,进一步优选为聚酰胺树脂。另外,热塑性树脂可以为一种,也可以为两种以上。
作为光吸收性树脂组合物中使用的聚酰胺树脂,对其种类等没有限定,优选为上述的结晶性热塑性树脂。
增强填料可示例出玻璃纤维、碳纤维、二氧化硅、氧化铝、炭黑及包覆有吸收激光的材料的无机粉末等能够吸收激光的填料,优选为玻璃纤维。玻璃纤维与可以配合在上述本实施方式的树脂组合物中的玻璃纤维含义相同。增强填料的含量优选为20~70质量%,更优选为25~60质量%,进一步优选为30~55质量%。
作为光吸收性色素,包含在待照射的激光波长的范围具有吸收波长的色素,例如,在本实施方式中,是在波长900nm~1100nm的范围具有吸收波长的色素。另外,光吸收性色素中包含如下色素:例如,相对于结晶性热塑性树脂100质量份配合0.3质量份、且在按照后面说明的实施例中记载的测定方法测定透光率时透射率小于30%、进而为10%以下的色素。
作为光吸收性色素的具体例,可列举无机颜料(炭黑(例如,乙炔黑、灯黑、热裂法炭黑、炉法炭黑、槽法炭黑、科琴黑等)等黑色颜料、氧化铁红等红色颜料、钼橙等橙色颜料、氧化钛等白色颜料)、有机颜料(黄色颜料、橙色颜料、红色颜料、蓝色颜料、绿色颜料等)等。其中,无机颜料通常遮盖力强,因此优选,进一步优选黑色颜料。这些光吸收性色素也可以组合使用两种以上。相对于结晶性热塑性树脂100质量份,光吸收性色素的含量优选为0.01~30质量份。
在上述组合物组合中,关于树脂组合物中除透光性色素及增强填料以外的成分和光吸收性树脂组合物中除光吸收性色素及增强填料以外的成分,优选80质量%以上是共通的,更优选90质量%以上是共通的,更进一步优选95~100质量%是共通的。
<<激光熔敷方法>>
接下来,对激光熔敷方法进行说明。在本实施方式中,可以对将由本实施方式的树脂组合物形成的成型品(透射树脂构件)与由上述光吸收性树脂组合物形成的成型品(吸收树脂构件)进行激光熔敷来制造成型品。通过进行激光熔敷,可以不使用粘接剂而将透射树脂构件与吸收树脂构件牢固地熔敷。
构件的形状没有特别限制,由于通过激光熔敷将构件彼此接合而使用,因此,通常为至少具有面接触部位(平面、曲面)的形状。在激光熔敷中,透过透射树脂构件的激光被吸收树脂构件吸收,吸收树脂构件熔融,将两个构件熔敷。特别是吸收树脂构件熔融,传热至透射构件,将两构件熔敷。由本实施方式的树脂组合物形成的成型品对激光的透射性高,因此可以优选用作透射树脂构件。这里,透射激光的构件的厚度(透射激光的部分沿激光透射方向的厚度)可以考虑用途、树脂组合物的组成及其它而适当确定,例如为5mm以下,优选为4mm以下。
作为激光熔敷中使用的激光光源,可以根据光吸收性色素的光的吸收波长来确定,优选为波长900~1100nm的范围的激光,例如可以利用半导体激光或光纤激光。
更具体而言,例如,在将透射树脂构件与吸收树脂构件熔敷的情况下,首先使两者待熔敷的部位彼此相互接触。此时,两者的熔敷部位优选为面接触,可以是平面与平面、曲面与曲面、或者平面与曲面的组合。接着,从透射树脂构件侧照射激光。此时,可以根据需要利用透镜将激光聚焦于两者的界面。该聚光射束透射至透射树脂构件中,在吸收树脂构件的表面附近被吸收而发热,发生熔融。接着,该热通过热传递也被传递至透射树脂构件,在两者的界面形成熔融池,在冷却后,将两者接合。
如上所述将透射树脂构件与吸收树脂构件熔敷而成的成型品具有高熔敷强度。需要说明的是,本实施方式的成型品除了包含完成品、部件以外,还包含形成它们的一部分的构件。
本实施方式中进行激光熔敷而得到的成型品的机械强度良好,具有高熔敷强度,因激光照射导致的树脂损伤也少,因此可以应用于例如各种保存容器、电气/电子设备部件、办公自动化(OA)设备部件、家电设备部件、机械装置部件、车辆装置部件等各种用途。特别可以优选用于食品用容器、药品用容器、油脂产品容器、车辆用中空部件(各种容器、进气歧管部件、照相机壳体等)、车辆用电气部件(各种控制单元、点火线圈部件等)电动机部件、各种传感器部件、连接器部件、开关部件、电流断路器部件、继电器部件、线圈部件、变压器部件、灯部件等。本发明的树脂组合物及组合物组合特别适于车载照相机模块。特别地,由本实施方式的树脂组合物及组合物组合形成的车载相机部件适于车载相机。
实施例
以下,列举实施例对本发明更具体地进行说明。只要不脱离本发明的主旨,以下的实施例中示出的材料、用量、比例、处理内容、处理步骤等可以适当变更。因此,本发明的范围并不限于以下所示的具体例子。
在实施例所使用的测定设备等因停产等而难以获取时,可以使用其它具有同等性能的设备进行测定。
<聚酰胺树脂>
MP10:间苯二甲基二胺/对苯二甲基二胺(M/P)摩尔比=7:3,按照下述合成例进行了合成。
<<MP10的合成例(M/P摩尔比=7:3)>>
将癸二酸在氮气氛围的反应罐内加热溶解后,一边对内容物进行搅拌,一边在加压(0.35MPa)下缓慢滴加对苯二甲基二胺(三菱瓦斯化学株式会社制)与间苯二甲基二胺(三菱瓦斯化学株式会社制)的摩尔比为3:7的混合二胺,使得二胺与癸二酸的摩尔比为约1:1,并且使温度上升至235℃。在滴加结束后,继续反应60分钟,调整了分子量1000以下的成分量。反应结束后,将内容物以线料状取出,用造粒机进行粒料化,得到了聚酰胺树脂(MP10)。
MP6:M/P摩尔比=7:3,按照下述合成例进行了合成。
<<MP6的合成例(M/P摩尔比=7:3)>>
将己二酸(RHODIA公司制)在氮气氛围的反应罐内加热溶解后,一边对内容物进行搅拌,一边在加压(0.35MPa)下缓慢滴加对苯二甲基二胺(三菱瓦斯化学株式会社制)与间苯二甲基二胺(三菱瓦斯化学株式会社制)的摩尔比为3:7的混合二胺,使得二胺与己二酸的摩尔比为约1:1,同时使温度上升至270℃。在滴加结束后,减压至0.06MPa,继续反应10分钟,调整了分子量1000以下的成分量。然后,将内容物以线料状取出,用造粒机进行粒料化,得到了聚酰胺树脂(MP6)。
PA66:聚酰胺66、INVISTA Nylon Polymer公司制、INVISTA U4800
<滑石>
#5000S:林化成株式会社制、Micron White
<碘化亚铜(CuI)>
日本化学产业株式会社制、Copper(I)iodide
<碘化钾>
Fuji Film Wako Pure Chemical Industries公司制
<硬脂酸锌(II)>
Fuji Film Wako Pure Chemical Industries公司制
<脱模剂>
CS8CP:日东化成工业株式会社制、褐煤酸皂
<氧化铈>
氧化铈1:纯度90质量%以上的氧化铈、Treibacher Industrie Japan公司制、Cerium Oxide Hydrate 90、铈含量72.1质量%、镧含量4.4质量%、中值粒径(基于激光衍射散射法的粒度)2μm以下
氧化铈2:纯度90质量%以上的氧化铈、Treibacher Industrie Japan公司制、Cerium Hydrate 90、铈含量78.5质量%、镧含量0.1质量%、中值粒径(基于激光衍射散射法的粒度)3μm以下
<氧化铈中的镧及铈含量分析>
将试样在大气中以120℃加热干燥2小时。精密称量试样100mg,添加高氯酸、双氧水及水,加温分解后,添加水而达到一定容量。将该溶液稀释,通过ICP发光分析法(ICP-AES),利用酸浓度匹配校准曲线法对Ce进行定量,并利用标准添加校准曲线法对La进行定量。
<透光性色素>
Lumogen 4281(K0088):BASF Color&Effect Japan株式会社制、苝颜料、Lumogen(注册商标)Black K 0088(旧名Lumogen Black FK 4281)
LTW-8701H:Orient Chemical Industries公司制、SolventRed179 0.46质量%、SolventYeloLw163 0.23质量%、AcidBlue80 6.53质量%
LTW-8731H:Orient Chemical Industries公司制、SoventRed179 1.56质量%、AcidBlue80 4.48质量%
<增强填料>
ECS03T-211H:E玻璃的玻璃纤维、日本电气硝子株式会社制、重均纤维径10.5μm、切断长度3.5mm
实施例1
<化合物>
以成为后述的表1所示的组成方式(表1的各成分为质量份表示)分别称量除增强填料以外的成分,使用双轴螺杆式盒式称重加料器(KUBOTA公司制、CE-W-1-MP)从双螺杆挤出机(东芝机械株式会社制、TEM26SS)的螺杆根部投入。另外,对于增强填料,使用振动式盒型称重加料器(KUBOTA公司制、CE-V-1B-MP)从挤出机的侧面投入上述的双螺杆挤出机,与树脂成分等进行熔融混炼,得到了树脂组合物粒料。挤出机的温度设定为280℃。
将上述得到的粒料以120℃干燥4小时后,使用注塑成型机(日本制钢所制、夹紧压力50T注塑成型机J-50ADS)制作了基于ASTM D638标准的4号片(1.5mm厚)。
<在高温高湿下放置后的颜色迁移试验>
在实施例1中,除透光性色素以外,用其它成分同样地进行混合、挤出并进行注塑成型,制造了基于ASTM D638标准的4号片(1.5mm厚)(对象构件)。
将由实施例1中记载的树脂粒料得到的基于ASTM D638标准的4号片与上述对象构件重合,用夹具进行了固定。然后,在85℃、相对湿度85%的条件下,静置50小时及1000小时。静置后,通过肉眼观察确认有无透光性色素向对象构件的颜色迁移,区分成A~E的5个级别进行了评价。将未确认到颜色迁移的情况设为A,将颜色迁移最严重的情况设为E。判断时,将比较例2的激光熔敷物在85℃、相对湿度85%的条件下静置1000小时后的试验片的颜色迁移的程度设为D,并以此为基准进行了判断。评价由10名专家进行,以多数票来确定。
实施例2~36、比较例1~18
在实施例1中,将原料的配合量如表1~6所示进行了变更(表2~表6的各成分的量以质量份表示),得到了树脂组合物粒料、基于ASTM D638标准的4号片(1.5mm厚)。此时,对于挤出机的温度设定而言,在使用MP6作为聚酰胺树脂的情况下设为280℃,在使用PA66的情况下设为280℃。
与实施例1同样地进行了在高温高湿下放置后的颜色迁移试验。需要说明的是,在实施例2中,对象构件使用了在表中实施例2所记载的树脂组合物中除透光性色素以外其它同样地进行而得到的对象构件。需要说明的是,在实施例3中,对象构件使用了在实施例3中记载的树脂组合物中除透光性色素以外其它同样地进行而得到的对象构件。实施例4~36及比较例1~18也同样。
以上,树脂组合物中的镧量根据来自氧化铈的镧量而计算出。其它成分的镧量为检测限以下。
根据上述结果可以明确,本发明的树脂组合物有效地抑制了颜色迁移。相比之下,在使用了除具有苝骨架的透光性色素以外的色素的情况下,颜色迁移的程度高。
Claims (18)
1.一种激光熔敷用透光性树脂组合物,其相对于结晶性热塑性树脂100质量份包含:
增强填料10~120质量份、
具有苝骨架的透光性色素0.01~1.0质量份、以及
通过ICP发光分析法测得的镧的含量超过0质量%且为1质量%以下的氧化铈。
2.根据权利要求1所述的树脂组合物,其中,
所述树脂组合物中的镧的含量超过0质量ppm且为40质量ppm以下。
3.根据权利要求1所述的树脂组合物,其进一步包含铜化合物及卤化碱金属中的至少一种。
4.根据权利要求2所述的树脂组合物,其进一步包含铜化合物及卤化碱金属中的至少一种。
5.根据权利要求1所述的树脂组合物,其中
树脂组合物中所述氧化铈的含量为0.01~5质量%。
6.根据权利要求2所述的树脂组合物,其中
树脂组合物中所述氧化铈的含量为0.01~5质量%。
7.根据权利要求3所述的树脂组合物,其中
树脂组合物中所述氧化铈的含量为0.01~5质量%。
8.根据权利要求4所述的树脂组合物,其中
树脂组合物中所述氧化铈的含量为0.01~5质量%。
9.根据权利要求1~8中任一项所述的树脂组合物,其中,
所述结晶性热塑性树脂包含聚酰胺树脂。
10.根据权利要求9所述的树脂组合物,其中,
所述聚酰胺树脂包含来自二胺的结构单元和来自二羧酸的结构单元,来自二胺的结构单元的70摩尔%以上来自于苯二甲基二胺,来自二羧酸的结构单元的70摩尔%以上来自于碳原子数4~20的α,ω-直链脂肪族二羧酸。
11.根据权利要求1~8中任一项所述的树脂组合物,其中,
所述具有苝骨架的透光性色素为颜料。
12.根据权利要求9所述的树脂组合物,其中,
所述具有苝骨架的透光性色素为颜料。
13.根据权利要求10所述的树脂组合物,其中,
所述具有苝骨架的透光性色素为颜料。
14.一种组合物组合,其具有:
权利要求1~13中任一项所述的树脂组合物、以及
包含热塑性树脂和光吸收性色素的光吸收性树脂组合物。
15.一种成型品,其由权利要求1~13中任一项所述的树脂组合物或权利要求14所述的组合物组合形成。
16.根据权利要求15所述的成型品,其为车载相机部件。
17.一种车载相机,其包含权利要求16所述的成型品。
18.一种成型品的制造方法,该方法包括:
对由权利要求1~13中任一项所述的树脂组合物形成的成型品、以及由包含热塑性树脂和光吸收性色素的光吸收性树脂组合物形成的成型品进行激光熔敷。
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Application Number | Priority Date | Filing Date | Title |
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KR20230015883A (ko) | 2023-01-31 |
EP4159815A4 (en) | 2024-06-26 |
CN115667415A (zh) | 2023-01-31 |
WO2021241381A1 (ja) | 2021-12-02 |
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